A gradient flow tank steady-state peeled whole component NFC type orange juice and a preparation method thereof
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-07-07
- Publication Date
- 2026-08-11
AI Technical Summary
[0007]本发明要解决的技术问题是:针对去皮橙肉全组分橙汁在保留汁胞、果肉纤维、细胞壁颗粒和内源果胶时容易出现高黏度、颗粒团聚、沉降分层、口感不均一以及连续化加工困难的问题,提供一种将高压射流磨细化分散与后置梯度溢流槽稳态化组装相结合的去皮全组分NFC型橙汁制备方法
1、本发明以酶法去皮橙肉全组分为主体原料,区别于全果压榨高纤维NFC橙汁路线,也区别于带皮全果破碎加水稀释饮料路线,能够减少橙皮苦味和粗糙感风险,同时保留橙肉内源果胶、果肉纤维和细胞壁颗粒。
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Figure CN122536686A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of juice processing, and specifically relates to a gradient overflow tank stabilized peeled whole-component NFC orange juice and its preparation method. Background Technology
[0002] NFC orange juice typically emphasizes non-concentrated, natural flavor, and retention of nutrients. Regular NFC orange juice often employs processes such as filtration, centrifugation, homogenization, degassing, sterilization, and cold chain storage to improve taste and flowability. However, excessive removal of pulp fiber, cell wall particles, and juice sac fragments, especially after filtration, reduces dietary fiber content, pulpy texture, and some flavor carrying capacity.
[0003] Peel-free whole-component orange juice uses orange pulp (after peeling) as the main ingredient, which reduces the risk of bitterness, roughness, and unpleasant flavor from the peel, while preserving as much juice vesicles, pulp fiber, cell wall particles, endogenous pectin, flavonoids, and flavor components as possible. However, the peel-free whole-component orange juice system is characterized by high pulp content, high fiber content, and high colloidal particle size, which can easily lead to problems such as high viscosity, wide particle size distribution, sedimentation and stratification, uneven taste, and difficulties in continuous processing.
[0004] Domestic patents already exist related to orange juice, NFC (Not From Concentrate) fruit and vegetable juice, or beverages containing fruit pulp. For example, CN103948103A discloses a method for producing a novel fruit juice by mixing orange sacs and orange juice; CN108850736A discloses a processing method and compound orange juice based on ultra-high pressure technology; CN110367409B discloses the extraction, ingredient mixing, filtration, mild heat sterilization, filling, and cold sterilization processes for NFC fruit and vegetable juice. These solutions can improve the shelf life, sterilization, or ingredient stability of the juice, but they do not establish a stepwise stable assembly structure for the endogenous pectin, pulp fiber, cell wall particles, and aroma oil droplets after the whole-component pulp of enzymatically peeled oranges is refined by high-pressure jet.
[0005] High-pressure jet milling or high-pressure jet pulverization technology itself is an existing technology. For example, CN108783137A discloses a method for producing fruit and vegetable beverages by jet pulverizing coarse fruit and vegetable raw material pulp into fine pulp using a high-pressure jet mill; CN117598415A discloses a wet pulverization, deaeration, and high-pressure jet ultrafine pulverization process for low-bitterness stable whole-fruit navel orange pulp; CN112691425A discloses that high-pressure jet mills can be used for pulverization, emulsification, and homogenization in food processing. The above technologies indicate that high-pressure jet mills can be used as a means of refining and homogenizing fruit and vegetable pulps, but the whole-component juice after high-shear refining may still be in a metastable dispersed state, and may still re-aggregate, settle, or separate during storage.
[0006] Therefore, it is necessary to provide a peel-free, full-component NFC orange juice preparation method that differs from the whole-fruit pressing high-fiber NFC orange juice route and the whole-fruit crushing and water dilution beverage route with peel. This method would form a continuous and synergistic process involving enzymatic peeling, wet pre-crushing, viscosity adjustment, high-pressure jet milling, and post-gradient overflow stabilization, thereby solving the problem of the difficulty in simultaneously preserving all components and ensuring the stability of the final product. Summary of the Invention
[0007] The technical problem to be solved by this invention is: to address the issues of high viscosity, particle agglomeration, sedimentation and stratification, uneven taste, and difficulties in continuous processing of peeled orange pulp whole-component orange juice when retaining juice cells, pulp fibers, cell wall particles, and endogenous pectin. This invention provides a method for preparing peeled whole-component NFC-type orange juice that combines high-pressure jet milling and dispersion with post-gradient overflow trough stabilization assembly.
[0008] To address the aforementioned technical problems, this invention provides a method for preparing NFC-type orange juice with peeled and stabilized state via gradient overflow tank, comprising the following steps: S1. Oranges are peeled using an enzymatic method to obtain peeled orange pulp that retains juice vesicles, pulp fibers, cell wall particles, and endogenous pectin. S2. The peeled orange pulp is wet-pre-pulverized, and NFC orange juice base viscosity-adjusting liquid is added during and / or after pre-pulverization to mix and adjust viscosity, so as to obtain peeled whole component fruit pulp with the peeled orange pulp as the main component. S3. The peeled whole-component fruit pulp is subjected to high-pressure jet milling to refine and evenly disperse the juice cell fragments, pulp fibers, cell wall particles, endogenous pectin and aroma oil droplets in the peeled whole-component fruit pulp, thereby obtaining refined whole-component fruit juice. S4. The refined whole-component juice is introduced into a gradient overflow tank for stabilization treatment. The gradient overflow tank is provided with multiple overflow chambers connected by an upper overflow method along the juice flow direction. Each of the multiple overflow chambers includes at least a heating activation chamber, a guiding assembly chamber, and a cooling and shaping chamber. The multiple overflow chambers are respectively configured with temperature and pH control conditions to form a gradient temperature and gradient pH along the juice flow direction. The refined whole-component juice flows through the heating activation chamber, the guiding assembly chamber, and the cooling and shaping chamber in sequence by overflow, thereby causing the endogenous pectin, pulp fiber, cell wall particles, juice cell fragments, and aroma oil droplets to gradually assemble into a stable suspended network and be discharged from the cooling and shaping chamber to obtain stable peeled whole-component NFC orange juice.
[0009] In this invention, the NFC orange juice base viscosity refers to an orange juice-based liquid, primarily composed of NFC orange juice, used to reduce the viscosity of the whole-component pulp of peeled oranges. The NFC orange juice base viscosity is either NFC orange juice or a mixture of NFC orange juice and water. When the NFC orange juice base viscosity is a mixture of NFC orange juice and water, NFC orange juice accounts for more than 70% of the mass of the NFC orange juice base viscosity, and water is only used as an auxiliary viscosity-adjusting component, not as the main diluent. Therefore, the resulting product is called peeled whole-component NFC orange juice.
[0010] In step S1, the enzymatic peeling process involves enzymatically peeling the oranges to obtain peeled orange pulp that retains juice vesicles, pulp fibers, cell wall particles, and endogenous pectin. This step aims to remove the orange peel and reduce the risk of excessive intake of orange peel oils and bitter substances into the product, while preserving the endogenous pectin and cell wall materials in the orange pulp, providing a raw material basis for the subsequent formation of a pectin-fiber-particle suspension network.
[0011] In step S2, wet pre-grinding and viscosity adjustment, the peeled orange pulp is wet-grinded and mixed with NFC orange juice base viscosity adjuster to obtain a peeled whole-component fruit pulp with peeled orange pulp as the main component. The purpose of this step is twofold: firstly, wet pre-grinding reduces the size of the peeled orange pulp tissue, allowing juice vesicles, pulp fibers, and cell wall particles to form a pumpable pulp; secondly, the NFC orange juice base viscosity adjuster reduces the pulp viscosity, improving the stability of continuous feeding in the jet mill. Compared to using water as the main diluent, using NFC orange juice base viscosity adjuster maintains the orange juice's sugar-acid system, flavor base, and nutrient concentration, preventing the peeled whole-component juice from being processed into a regular diluted beverage.
[0012] In step S3, the high-pressure jet milling refinement process, the peeled whole-component fruit pulp is subjected to high-pressure jet milling to refine and uniformly disperse juice sac fragments, pulp fibers, cell wall particles, endogenous pectin, and aroma oil droplets, resulting in refined whole-component fruit juice. This step utilizes the physical effects of shearing, impact, cavitation, and instantaneous pressure drop generated by the high-pressure jet mill to refine the juice sac fragments, pulp fibers, and cell wall particles in the peeled whole-component fruit pulp, expose the surface structure of endogenous pectin and pulp fibers, and uniformly disperse aroma oil droplets, thereby forming a refined whole-component fruit juice suitable for subsequent gradient overflow tank stabilization assembly.
[0013] In step S4, the gradient overflow stabilization step, the refined whole-component juice is introduced into the gradient overflow trough. The gradient overflow trough is provided with multiple overflow chambers connected by an upper overflow mechanism along the juice flow direction. These overflow chambers include at least a heating activation chamber, a guiding assembly chamber, and a cooling and shaping chamber. The purpose of this step is to transform the metastable dispersed state after high-pressure jet milling into a stable suspended network, preventing coarse pulp from directly entering the guide trough and causing blockage, and also preventing the network formed in the guide trough from being further damaged by subsequent strong shearing.
[0014] The stable suspension network referred to in this invention refers to the suspended dispersion structure formed by juice cell fragments, pulp fibers, cell wall particles, endogenous pectin, and aroma oil droplets after high-pressure jet milling, under the action of gradient overflow in the upper part of a gradient overflow tank, gradient temperature, gradient pH, and optional low-intensity pulsed ultrasound. This stable suspension network can be characterized by one or more of the following indicators: LUMiFuge instability index, static stratification index, centrifugal sedimentation rate, and particle size distribution. Preferably, under the LUMiFuge test conditions of a detection wavelength of 865 nm, a rotation speed of 3000 r / min, a temperature of 25 °C, a sampling interval of 10 s, sampling of 300 sets of spectra, and a total detection time of 2990 s, the instability index of the peeled whole-component NFC-type orange juice is not higher than 0.30, more preferably not higher than 0.22.
[0015] Preferably, the temperature of the heating activation chamber is 35℃-55℃, and the pH is 3.3-4.0. Its function is to reduce the viscosity of the juice system, promote the activity of endogenous pectin segments, and facilitate contact between pulp fibers and cell wall particles. The temperature of the guiding assembly chamber is 20℃-40℃, and the pH is 3.6-4.5. Its function is to promote the formation of a networked suspension structure of endogenous pectin, pulp fibers, cell wall particles, juice sac fragments, and aroma oil droplets under overflow thin-layer and guided flow conditions. The temperature of the cooling and setting chamber is 4℃-25℃, and the pH is 3.4-4.2. Its function is to cool and set the already formed networked suspension structure, reducing the risk of re-aggregation and sedimentation stratification.
[0016] Preferably, the gradient overflow tank may further include an inlet buffer chamber, the temperature of which is 15℃-45℃ and the pH is 3.0-4.5. The inlet buffer chamber is used to buffer the fluctuations in feed pressure, flow rate and temperature after the high-pressure jet mill discharge, and to reduce the local turbulence and uneven feeding caused by the direct impact of the jet discharge on the heating activation chamber.
[0017] Preferably, an overflow weir is provided between two adjacent overflow chambers, so that after the whole component juice reaches a predetermined liquid level in the previous overflow chamber, it crosses the corresponding overflow weir and enters the next overflow chamber. The overflow weir can form a weir crest height that gradually decreases along the juice flow direction, or a liquid level difference can be formed through the upper overflow port and overflow pipe, thereby controlling the residence time and thin overflow path in each overflow chamber.
[0018] Preferably, the height of the overflow weir plate decreases gradually along the direction of juice flow.
[0019] Preferably, the cooling and setting chamber is equipped with a discharge port, which is located on the side away from the inlet end of the cooling and setting chamber and is formed as a rounded, slow-flow discharge port. The set, peeled, full-component NFC orange juice is discharged through the rounded, slow-flow discharge port via gravity flow and / or a low-speed volumetric pump. This feature prevents the already formed suspended network from being disrupted by passing through high-shear equipment or abruptly narrowed pipes during the discharge stage.
[0020] Preferably, the inlet buffer chamber, heating activation chamber, guiding assembly chamber, and cooling and shaping chamber can all be equipped with pH monitors, pH adjustment ports, temperature monitors, and temperature control devices. The pH can be adjusted using food-grade acids such as citric acid, citrate, malic acid, and malate, food-grade salts, or their buffer systems. This feature ensures that the temperature and pH parameters are controllable within the natural acidity range of orange juice, preventing significant changes in the orange juice flavor.
[0021] Preferably, the gradient overflow tank may also be equipped with an ultrasonic auxiliary unit. The ultrasonic auxiliary unit includes an insertable ultrasonic probe and / or an externally coupled ultrasonic transducer. The insertable ultrasonic probe includes an amplitude transformer and an ultrasonic tool head, which extends below the working liquid surface of the corresponding overflow chamber to directly apply low-intensity or pulsed ultrasound to the juice system. The externally coupled ultrasonic transducer is disposed on the tank wall, tank bottom, or external jacket of the corresponding overflow chamber to couple and transmit ultrasonic energy to the juice system through the tank wall, tank bottom, or external jacket. The insertable ultrasonic probe and the externally coupled ultrasonic transducer can be used individually or in combination.
[0022] The ultrasonic-assisted unit does not replace the high-pressure jet mill for secondary strong shearing and pulverization, but rather prevents the deposition of pulp fibers, cell wall particles, and juice cell fragments in the inlet buffer chamber, heating activation chamber, and guiding assembly chamber, promotes the contact between endogenous pectin and pulp fibers, cell wall particles, and aroma oil droplets, and improves the uniformity of the overflow thin layer.
[0023] The present invention further specifies the preferred process parameters: the ratio of oranges to enzymatic hydrolysate is 1:2-3, the pH of the enzymatic hydrolysate is 3.5-4.5, the amount of enzyme added is 1‰-4‰ of the mass of the enzymatic hydrolysate, and the enzymatic peeling time is 40min-60min; the wet pre-pulverization is preferably a two-stage wet pre-pulverization, with the rotation speed of both the first and second stages being 3000r / min-5000r / min, preferably 4000r / min; the mass percentage of NFC orange juice in the NFC orange juice base viscosity is not less than 50%, preferably not less than 70%; the high-pressure jet milling treatment pressure is 60MPa-120MPa, preferably 80MPa-120MPa, and more preferably 90MPa-110MPa.
[0024] Furthermore, the preparation method may also include steps or structures such as raw material cleaning and selection, post-peeling residual skin handling, low-temperature temporary storage, online degassing, pasteurization, low-temperature sterilization, ultra-high pressure sterilization, aseptic filling, cold chain filling, online CIP cleaning, temperature / pH closed-loop control, low-shear conveying, and continuous multi-channel parallel overflow tanks. These features can be selected according to the production line requirements.
[0025] This invention also provides a peeled, full-component, NFC-type orange juice, prepared by the above method, containing a stable suspension network formed by endogenous pectin, pulp fiber, cell wall particles, juice sac fragments, and aroma oil droplets. This product can be used as a pulp-containing, stable orange juice or a non-therapeutic dietary fiber supplement.
[0026] The beneficial effects of this invention are as follows: 1. This invention uses enzymatically peeled orange pulp as the main raw material, which is different from the whole fruit pressing high-fiber NFC orange juice route and also different from the whole fruit crushing and water dilution beverage route with peel. It can reduce the risk of bitterness and roughness of orange peel, while retaining the endogenous pectin, pulp fiber and cell wall particles of orange pulp.
[0027] 2. This invention reduces the viscosity of the fruit pulp by wet pre-crushing and mixing with NFC orange juice base viscous liquid, thereby improving the continuous pumping stability of peeled whole-component fruit pulp and the feeding stability of high-pressure jet mill.
[0028] 3. In this invention, the high-pressure jet mill is set as the refining and dispersing step, and the gradient overflow tank is set as the post-stabilization step, forming a continuous process chain of refining and dispersing first, and then low-shear assembly and shaping.
[0029] 4. This invention uses gradient temperature, gradient pH and optional low-intensity pulsed ultrasound to gradually form a stable suspension network of refined endogenous pectin, pulp fiber, cell wall particles, juice cell fragments and aroma oil droplets, which is beneficial to improve sedimentation stratification and taste consistency. Attached Figure Description
[0030] A brief explanation of the contents of each figure in the instruction manual and the markings in the figures is provided: Figure 1 This is a schematic diagram of the gradient overflow stabilization preparation process for peeled, full-component NFC-type orange juice in Example 1.
[0031] Figure 2 This is a schematic diagram of the specific structure of the gradient overflow channel in Example 1.
[0032] Figure 3 This is a schematic diagram of the cooling and shaping chamber discharge and low-shear discharge structure in Example 1.
[0033] Figure 4This is a schematic diagram illustrating the step-by-step assembly mechanism of peeled whole-component fruit juice in an example.
[0034] Figure 5 This is a graph showing the static stability of peeled, full-component NFC-type orange juice from Experiment Example 1.
[0035] Figure 6 The figure shows the LUMiFuge stability test results of peeled, full-component NFC orange juice under the steady-state conditions of different gradient overflow tanks in Experiment Example 2.
[0036] Figure 7 The figure shows the LUMiFuge stability verification test results of peeled whole-component NFC orange juice under different stabilization treatments in Experiment Example 3.
[0037] Figure 8 The graph shows the instability index evaluation of samples with different jet pressures in Experiment Example 4.
[0038] Figure 9 This is an evaluation chart of the average particle size of samples with different jet pressures in Experiment Example 4.
[0039] Figure 10 This is an evaluation chart of dietary fiber-related indicators for the peeled whole-component orange juice in Experiment Example 5. Detailed Implementation
[0040] The present invention will now be further described with reference to the accompanying drawings and specific embodiments. It should be noted that, without conflict, the various embodiments or technical features described below can be arbitrarily combined to form new embodiments. Unless otherwise specified, the raw materials, equipment, etc., used in the following embodiments can all be obtained by purchase.
[0041] Example 1: Complete Production Process of Peeled, Full-Component NFC Orange Juice like Figure 1 As shown, this embodiment uses oranges from the same origin, with basically uniform ripeness, no mold, and no obvious mechanical damage as raw materials, and is described based on 100kg of oranges. Newhall navel oranges, tangerines, blood oranges, Late Luncia oranges, or other sweet orange varieties suitable for juicing are preferred. Newhall navel oranges were used in this embodiment and other experimental examples.
[0042] S1, Raw material cleaning and selection. 100kg of oranges are sprayed or bubbled to remove surface mud and impurities, and rotten, diseased, insect-infested, and obviously mechanically damaged fruits are removed. After draining, they are put into the enzymatic peeling device.
[0043] S2. Prepare the enzymatic hydrolysate. Prepare 250 kg of enzymatic hydrolysate at a ratio of oranges to hydrolysate of 1:2.5. Adjust the pH of the hydrolysate to 4.0 using food-grade citric acid and sodium citrate. Add food-grade compound citrus peeling enzyme to the hydrolysate at a concentration of 3‰ of the hydrolysate mass. The compound citrus peeling enzyme includes pectinase, cellulase, and hemicellulase.
[0044] S3, Enzymatic Peeling. Washed oranges are added to an enzymatic hydrolysate, ensuring the oranges are fully submerged. The enzymatic treatment temperature is controlled at 45℃, and the soaking time is 50 minutes. Subsequently, the oranges are mechanically peeled using a peeling machine, resulting in peeled orange pulp that retains juice vesicles, pulp fibers, cell wall granules, and endogenous pectin. The applicant filed patent CN202210384098.X on April 12, 2022, for a process, equipment, and application of enzymatic peeling and desquamation of citrus fruits. Enzymatic peeling can be performed using this process.
[0045] S4, Orange Segment Preparation. Spray the peeled orange segments with a small amount of NFC orange juice to remove residual peel fragments, and discard any obvious remaining peel, stems, and browned tissue. This step does not involve acid-base desquamation or filtration to remove pulp fibers, cell wall particles, or juice sac fragments.
[0046] S5, Wet primary pre-grinding. Peeled orange pulp is continuously added to the primary wet pre-grinding equipment at a speed of 4000 r / min to obtain primary pulverized pulp. This step breaks the peeled orange pulp into a pumpable state, preventing large pieces of orange pulp from directly entering the high-pressure jet mill and causing blockage.
[0047] S6, Wet secondary pre-grinding. The fruit pulp from the primary grinding enters the secondary wet pre-grinding equipment, with the rotation speed set at 4000 r / min, to obtain the secondary ground fruit pulp. The secondary grinding is used to further disperse the juice vesicle tissue and pulp fiber, so that the fruit pulp has a relatively uniform flow state before entering the jet storage tank.
[0048] S7, Mixing NFC orange juice base viscous liquid. Add NFC orange juice to the secondary-crushed pulp at a 1:1 mass ratio and mix to obtain a peeled, full-component pulp. If the raw material batch has a high viscosity, a mixture of NFC orange juice and water can be used as the NFC orange juice base viscous liquid, but the NFC orange juice should account for at least 70% of the NFC orange juice base viscous liquid by mass. In this embodiment, NFC orange juice is used as the sole NFC orange juice base viscous liquid, and no water is added.
[0049] S8, High-Pressure Jet Milling. The viscous, peeled, whole-component fruit pulp is fed into a jet storage tank and then pumped into a high-pressure jet mill. The high-pressure jet mill is set to a processing pressure of 100 MPa, and the process is repeated once. During the process, the discharge temperature is controlled to not exceed 45°C through cooling. After processing, a refined whole-component juice is obtained, in which juice cell fragments, pulp fibers, cell wall particles, endogenous pectin, and aroma oil droplets are in a refined and dispersed state. In this embodiment, an AMH-1000 pilot-scale microjet homogenizer is used as the high-pressure jet mill. Other equivalent equipment capable of continuous high-pressure jet refining of fruit and vegetable pulp within a pressure range of 60 MPa-120 MPa can also be used.
[0050] S9, Gradient Overflow Tank Stabilization. The refined whole-component juice processed by the high-pressure jet mill is introduced into the gradient overflow tank, where it sequentially passes through the inlet buffer chamber, the heating activation chamber, the guiding assembly chamber, and the cooling and shaping chamber. This step transforms the metastable dispersion system after the high-pressure jet mill into a stable suspended network.
[0051] S10, Post-processing and Filling. After being discharged from the cooling and shaping chamber, the peeled, full-component NFC orange juice is temporarily stored at low temperature, degassed, sterilized at low temperature or under ultra-high pressure, and then aseptically filled or filled in a cold chain.
[0052] After stabilization treatment in a gradient overflow tank, the peeled, full-component NFC-type orange juice can be placed in a low-temperature temporary storage tank, preferably at a temperature of 0°C to 10°C. If dissolved oxygen needs to be reduced, vacuum degassing or ultrasonic-assisted degassing can be performed under low-temperature conditions. After degassing, the juice should proceed to the sterilization or filling stage as soon as possible. Sterilization methods can include low-temperature pasteurization, short-time heat sterilization, ultra-high pressure sterilization, or other cold sterilization methods suitable for NFC orange juice. If heat sterilization is used, the heat load should be controlled to avoid damaging the pectin-fiber suspension network and aroma components. If ultra-high pressure sterilization is used, it can be placed at a suitable location after or before filling. Filling methods can include aseptic filling, cold chain filling, or filling with sterilized packaging materials. After filling, the product can be refrigerated at 0°C to 4°C, or its shelf life can be evaluated according to the sterilization method and packaging conditions. Table 1 shows the parameter selection in the preparation method of peeled, full-component NFC-type orange juice in this embodiment.
[0053]
[0054] Table 1. Parameters for the Preparation Method of Peeled, Full-Component NFC Orange Juice like Figure 2The diagram shows a schematic of a gradient overflow tank. The gradient overflow tank includes an inlet buffer chamber, a heating activation chamber, a guiding assembly chamber, and a cooling and shaping chamber, arranged sequentially along the flow direction of the juice and connected by an upper overflow mechanism. An overflow weir plate is installed between adjacent overflow chambers. In this embodiment, the crest height of the first overflow weir plate is higher than that of the second overflow weir plate, and the crest height of the second overflow weir plate is higher than that of the third overflow weir plate, forming a decreasing weir crest height along the flow direction. This allows the juice to cross the corresponding overflow weir plate and enter the next overflow chamber after reaching a predetermined liquid level in the previous overflow chamber.
[0055] The inlet buffer chamber is connected to the outlet of the high-pressure jet mill and is used to buffer the flow rate and pressure fluctuations caused by the discharge from the high-pressure jet mill. In this embodiment, the temperature of the inlet buffer chamber is controlled at 25°C, the pH is controlled at 3.8, and the residence time is 45s. The heating and activation chamber is equipped with a temperature control device, a pH adjustment port, a pH monitor, and a temperature monitor. In this embodiment, the temperature of the heating and activation chamber is controlled at 45°C, the pH is controlled at 3.6, and the residence time is 120s. This chamber is used to reduce the viscosity of the juice system, improve the activity of endogenous pectin segments, and promote the contact between pulp fibers and cell wall particles. After the juice reaches the predetermined liquid level of the first overflow weir in the heating and activation chamber, it crosses the overflow weir in a thin layer and enters the guide assembly chamber. In this embodiment, the temperature of the guide assembly chamber is controlled at 32°C, the pH is controlled at 4.0, and the residence time is 180s. This chamber, through thin-layer overflow, tank geometry guidance, and temperature-pH coupling, allows endogenous pectin, pulp fibers, cell wall particles, juice cell fragments, and aroma oil droplets to gradually form a networked suspension structure. After the juice reaches the predetermined level on the second overflow weir in the guiding assembly chamber, it enters the cooling and shaping chamber. In this embodiment, the temperature of the cooling and shaping chamber is controlled at 12°C, the pH is controlled at 3.8, and the residence time is 180s. This chamber is used to reduce the risk of particle re-aggregation and network damage, and to stabilize the suspended network formed in the guiding assembly chamber 403. Specific parameters are shown in Table 2.
[0056] The pH in each overflow chamber is finely adjusted using a food-grade citric acid and sodium citrate buffer system. Each overflow chamber is equipped with a temperature monitor and a pH monitor, and the temperature control device and pH adjustment port are adjusted via a controller to keep the temperature and pH within the set range.
[0057]
[0058] Table 2 Temperature and pH control conditions for each overflow chamber like Figure 3 As shown, the outlet of the cooling and setting chamber is located on the side away from the inlet of the cooling and setting chamber, allowing the juice to have sufficient residence time in the cooling and setting chamber before being discharged. A flow buffer can be installed in the cooling and setting chamber to extend the flow path and avoid short-circuit flow where the juice is discharged directly from the outlet as soon as it enters the cooling and setting chamber.
[0059] The discharge port is preferably a rounded, slow-flow discharge port, forming a smooth transition structure between the discharge port and the bottom or side wall of the cooling and shaping chamber to avoid abrupt diameter reduction and localized high-speed impact. The discharge port is connected to a food-grade discharge pipeline, and the average flow velocity of the juice in the pipeline is controlled at 0.3 m / s.
[0060] In this embodiment, the shaped, peeled, full-component NFC orange juice is discharged by gravity flow due to liquid level difference. When pumping is required, a low-speed cam rotor pump is used to assist in the discharge, with a pump speed of 80 r / min. During the discharge process, it no longer passes through a high-pressure jet mill, high-speed homogenizer, high-speed centrifugal pump, throttling nozzle, or high-speed agitator to avoid damaging the stable suspension network formed after cooling and shaping.
[0061] like Figure 2 As shown, an ultrasonic auxiliary unit can be further installed in the gradient overflow tank. In this embodiment, ultrasonic auxiliary units are respectively installed in the inlet buffer chamber, the heating activation chamber, and the guide assembly chamber. The ultrasonic auxiliary unit can be an insertion-type ultrasonic probe or an externally coupled ultrasonic transducer. When using an insertion-type ultrasonic probe, the probe includes an amplitude transformer and an ultrasonic tool head. The ultrasonic tool head, as the sound output end, extends below the working liquid surface of the corresponding overflow chamber, with the insertion depth ensuring that the sound output end is covered by the juice and does not contact the bottom of the tank. When using an externally coupled ultrasonic transducer, the transducer is fixed to the tank wall, bottom, or external jacket of the corresponding overflow chamber, transmitting ultrasonic energy to the juice system through the tank wall or jacket. This embodiment uses an insertion-type ultrasonic probe.
[0062] In this embodiment, the inlet buffer chamber uses pulsed ultrasound at 25 kHz, a sound power density of 0.08 W / cm², and a duty cycle of 10%. The use of low-intensity pulsed ultrasound in the inlet buffer chamber prevents rapid deposition of pulp fibers and cell wall particles at the bottom of the tank after the high-pressure jet mill discharge. The heating activation chamber uses pulsed ultrasound at 28 kHz, a sound power density of 0.18 W / cm², and a duty cycle of 20%. The use of low to medium intensity pulsed ultrasound in the heating activation chamber promotes contact between pectin, fibers, and cell wall particles. The guiding assembly chamber uses pulsed ultrasound at 35 kHz, a sound power density of 0.35 W / cm², and a duty cycle of 35%. The use of relatively high but still low intensity pulsed ultrasound in the guiding assembly chamber promotes the homogenization of the overflow thin layer and the formation of the suspended network. The cooling and shaping chamber typically shuts off the ultrasound or uses only very low-intensity disturbances to avoid damaging the already formed networked suspended structure. Specific functions and parameters are shown in Table 3.
[0063] Each ultrasonic auxiliary unit is linked to the temperature monitor of its corresponding overflow chamber for control. When the juice temperature in the corresponding overflow chamber exceeds the set upper temperature limit of 1℃-3℃, the controller reduces the output power of the corresponding insertion ultrasonic probe or externally coupled ultrasonic transducer, or suspends ultrasonic output. This linkage control is used to avoid local temperature rise, vitamin C loss, aroma substance volatilization, or damage to the suspended network caused by ultrasound.
[0064] Each transducer is linked to the temperature monitor of its corresponding overflow chamber for control. When the juice temperature in the corresponding overflow chamber exceeds the set upper temperature limit of 2°C, the output power of the corresponding transducer is reduced or the ultrasonic output is paused. This control method is used to avoid localized temperature rise, aroma loss, or damage to the suspension network caused by ultrasound.
[0065]
[0066] Table 3 Parameter List of Ultrasonic Assisted Unit like Figure 4 As shown, in the refined whole-component juice processed by high-pressure jet milling, pulp fibers, endogenous pectin, cell wall particles, juice cellular fragments, and aroma oil droplets are in a refined dispersed state. This dispersed state is beneficial for reducing particle size and improving homogeneity; however, without subsequent stabilization and solidification, the dispersed phase may still re-aggregate, settle, or stratify. In a gradient overflow tank, the refined whole-component juice undergoes sequential heating activation, guided assembly, and cooling solidification. Heating activation increases chain segment mobility and reduces viscosity; guided assembly utilizes thin-layer overflow and pH fine-tuning to promote the formation of a network of pectin, fibers, particles, and oil droplets; cooling solidification reduces the risk of molecular motion and particle re-aggregation, thereby forming a stable suspended network.
[0067] Experimental Example 1: Observation of the static stability of 1:1 diluted, peeled, full-component NFC orange juice. This experiment was used to evaluate the natural static stability of 1:1 viscous, peeled, full-component NFC orange juice after different high-pressure jet milling pressures and post-gradient overflow tank treatments. At the same time, a sample treated with 100MPa high-pressure jet milling but without gradient overflow tank treatment was set up as a comparative example to verify the role of gradient overflow tank in the formation of a stable suspended network.
[0068] I. Preparation of Experimental Samples All experimental samples used the same batch of oranges as raw materials and were processed according to S1 to S9 of Example 1: the pH of the enzymatic hydrolysate was 4.0, the ratio of oranges to enzymatic hydrolysate was 1:2.5, the amount of enzyme added was 3‰ of the mass of the enzymatic hydrolysate, and the enzymatic peeling time was 50 min; the peeled orange pulp was subjected to primary wet pre-pulverization and secondary wet pre-pulverization in sequence, and the rotation speed of primary wet pre-pulverization and secondary wet pre-pulverization was 4000 r / min; the resulting secondary pulverized pulp was mixed with NFC orange juice at a mass ratio of 1:1 to adjust the viscosity, resulting in a 1:1 adjusted viscosity peeled whole component pulp.
[0069] The 1:1 viscosity-adjusted peeled whole-component fruit pulp was divided into five groups for treatment. Each group of samples was... Figure 5 Each sub-image is arranged in the same order from left to right, as shown in Table 4.
[0070]
[0071] Table 4 Sample setup and bottle position correspondence for static stability observation in Experiment Example 1 Among them, samples S-1 to S-4, after being treated once each by high-pressure jet milling at 120MPa, 100MPa, 80MPa, and 60MPa respectively, all continued to enter the post-gradient overflow tank and underwent stabilization treatment according to the gradient overflow tank treatment conditions in Example 1: inlet buffer chamber temperature 25℃, pH 3.8, residence time 45s; heating activation chamber temperature 45℃, pH 3.6, residence time 120s; guiding assembly chamber temperature 32℃, pH 4.0, residence time 180s; cooling and shaping chamber temperature 12℃, pH 3.8, residence time 180s. The only difference between sample D-1 and sample S-2 is that sample D-1, after being treated by high-pressure jet milling at 100MPa, did not enter the gradient overflow tank, but was directly cooled to the same filling temperature as sample S-2 before filling.
[0072] II. Static Observation Method Samples S-1, S-2, S-3, S-4, and D-1 were separately filled into identical transparent observation vials, ensuring a consistent liquid level in each vial. After filling, each sample was gently inverted three times to mix thoroughly, and then placed vertically in a dark environment at room temperature. The sample vials were not shaken before photography, and images were acquired using a fixed light source, background, and shooting distance.
[0073] The observation time points were set sequentially as 0h, 4h, 8h, 1d, 2d, 3d, 4d, 5d, 6d, 7d, 29d, 30d, and 31d. Figure 5 The subgraphs are arranged in order of resting time; in each subgraph, from left to right, they are S-1, S-2, S-3, S-4 and D-1.
[0074] III. Evaluation Methods The stability of the sample under static conditions was observed and evaluated using the following indicators: First, observe whether a clear layer forms on top of the sample; second, observe whether a dense sediment layer forms at the bottom of the sample; third, observe whether the turbidity and color in the middle of the sample are continuous and uniform; fourth, compare whether the stratification interface of each sample is clear after prolonged static conditions. The less clear layer at the top, the thinner the dense sediment at the bottom, and the more uniform the turbidity in the middle, the more stable the suspended network formed by endogenous pectin, pulp fiber, cell wall particles, juice sac fragments, and aroma oil droplets in the sample.
[0075] When a semi-quantitative evaluation is required, the static stratification index can be calculated using the following formula: Separation index = (height of upper clear layer + height of bottom sediment layer) / total liquid column height of sample × 100%.
[0076] The smaller the static stratification index, the better the sample stability; correspondingly, the suspension retention rate = 1 - static stratification index, and the higher the suspension retention rate, the more stable the suspended network.
[0077] IV. Observation Results like Figure 5 As shown, within 0h to 8h, the four samples S-1, S-2, S-3, and S-4 treated in the gradient overflow tank exhibited a uniform overall appearance, with no obvious upper clarification layer or dense bottom sedimentation observed. This indicates that the 1:1 viscosity-adjusted samples treated with high-pressure jet milling (60MPa to 120MPa) followed by gradient overflow tank stabilization all possessed initial suspension stability. Sample D-1 also exhibited some uniformity in the initial stage, but its suspension state mainly stemmed from the fine dispersion achieved by the high-pressure jet milling and had not yet formed a stable suspension network stabilized by the gradient overflow tank.
[0078] After standing for 1 to 7 days, samples S-1, S-2, S-3, and S-4 maintained good overall turbidity continuity, with no significant separation between the upper and lower phases. Among them, sample S-2, which was treated by a 100MPa high-pressure jet mill followed by a gradient overflow tank, exhibited the most uniform turbidity in the middle, the least obvious clarification layer in the upper part, and the thinnest sediment layer at the bottom, demonstrating the best standing stability among the four gradient overflow tank-treated samples. Sample S-3 showed the second best stability. Although samples S-1 and S-4 did not show significant instability, their local turbidity uniformity and slight bottom sedimentation were slightly worse than those of S-2.
[0079] After standing for 29 to 31 days, the four samples (S-1, S-2, S-3, and S-4) treated with the gradient overflow tank did not show unacceptable severe stratification, indicating that the post-gradient overflow tank can enable the refined whole-component juice to form a stable suspension network under different jet pressures. Among the four samples, sample S-2 still showed continuous turbidity in the middle of the bottle, less clear layer at the top, and thin sedimentation layer at the bottom, indicating that the combination of 100MPa high-pressure jet milling and gradient overflow tank stabilization treatment is most conducive to the formation of a stable suspension network. Sample D-1 showed more obvious upper clarification and bottom sedimentation than sample S-2, indicating that although 100MPa high-pressure jet milling alone can achieve fine dispersion, the lack of low-shear assembly and cooling and shaping by the post-gradient overflow tank results in insufficient long-term stability.
[0080] V. Stability Analysis Samples S-1 to S-4 all showed stability, indicating that within a pressure range of 60 MPa to 120 MPa, the high-pressure jet mill can refine and disperse juice cell fragments, pulp fibers, cell wall particles, and aroma oil droplets in the peeled whole-component fruit pulp, providing a foundation for subsequent gradient overflow tank assembly. The heating activation chamber in the gradient overflow tank reduces system viscosity and increases the contact probability of endogenous pectin, pulp fibers, and cell wall particles; the guiding assembly chamber promotes pectin-fiber-particle-oil droplet overlap through thin-layer overflow and guided flow; and the cooling and setting chamber reduces particle re-aggregation and sedimentation rates, thereby further transforming the refined dispersed state into a stable suspended network state.
[0081] The reason why sample S-2 exhibits the best stability is that the 100MPa high-pressure jet mill achieves a good balance between particle refinement, exposure of endogenous pectin, and maintenance of the suspended network. At pressures as low as 60MPa, some pulp fibers and cell wall particles are insufficiently refined, resulting in a relatively inadequate foundation for subsequent assembly. While pressures as high as 120MPa can further reduce particle size, they may lead to excessive fragmentation or overly fine particle size distribution of some network-building components, thus failing to demonstrate a further stability advantage compared to the 100MPa sample. Therefore, a pressure of around 100MPa combined with a post-gradient overflow tank is the preferred process condition for preparing stable, peeled, full-component NFC-type orange juice in this application.
[0082] A comparison between S-2 and D-1 reveals that both utilize a 100MPa high-pressure jet mill, differing only in whether or not they undergo gradient overflow treatment. S-2 exhibits less upper clarification, thinner bottom sedimentation, and more uniform bottle turbidity compared to D-1. This indicates that the post-gradient overflow tank is not merely a conveying or cooling device, but rather a stabilization treatment unit that promotes the formation of a stable suspended network through gradient temperature, gradient pH, the upper overflow path, and cooling and shaping effects.
[0083] This experimental example is a static visualization observation experiment, used to illustrate the macroscopic stratification trend of samples under different high-pressure jet mill pressures and samples that have been treated with gradient overflow grooves under 1:1 viscosity adjustment conditions. Figure 5 The first four samples underwent gradient overflow stabilization treatment, and no unacceptable severe stratification occurred during the observation period. The sample treated with a 100MPa high-pressure jet mill followed by gradient overflow stabilization showed a smaller upper clarification layer, a thinner bottom sediment layer, and more uniform turbidity in the middle, demonstrating good static stability. Since static photographs are affected by shooting angle, lighting, and liquid column height, this experimental example is mainly used for macroscopic stability observation. The quantitative evaluation of suspension stability in this application is mainly completed using the LUMiFuge instability index of Experiments 2 and 3.
[0084] Experiment Example 2: Gradient Overflow Channel Process Screening Experiment Based on Example 1 The LUMiFuge stability test evaluated the suspension stability of the samples using centrifugation acceleration and near-infrared transmitted light monitoring. During the test, the samples were placed in a 2mm rectangular sample cell of a LUM and centrifuged at 3000 r / min and 25℃. The detection wavelength was 865 nm, with a sampling interval of 10 s, collecting 300 spectral lines for a total detection time of 2990 s. The test results are expressed as an instability index. A higher instability index indicates a faster change in sample transmittance, more pronounced particle migration, sedimentation, or stratification, and thus greater sample instability; a lower instability index indicates better sample suspension stability.
[0085] In the LUMiFuge test, the software was set to a detection time of 3000s and a data acquisition interval of 10s, acquiring a total of 300 sets of spectra. Since the software uses the initial time as the first set of data, the final time corresponding to the instability index in the results table is displayed as 2990s. Therefore, the "Set Detection Time / s" in the table is 3000s, and the "Test Time / s" is 2990s, which is not contradictory.
[0086] This experimental example is used to illustrate... Figure 6 How were the LUMiFuge stability data obtained? All samples were based on the refined whole-component juice obtained in S1 to S8 of Example 1, differing only in the stabilization treatment conditions after high-pressure jet milling. Sample numbers are internal numbers used in this experimental example.
[0087] The specific sample preparation methods are as follows: 1-1 is a sample that did not enter the gradient overflow tank after being milled at 100MPa high-pressure jet mill; 1-2 is a sample that entered the ordinary constant-height overflow tank after being milled at 100MPa high-pressure jet mill but without temperature and pH gradients; 1-3 is a sample that entered the constant-height overflow tank after being milled at 100MPa high-pressure jet mill and subjected to continuous ultrasound; 2-1 is a sample that entered the descending overflow tank after being milled at 100MPa high-pressure jet mill and with a temperature gradient but no pH gradient; 2-2 is a sample that entered the descending overflow tank after being milled at 100MPa high-pressure jet mill and with a pH gradient but no temperature gradient; 2-3 is a sample that entered the descending overflow tank after being milled at 100MPa high-pressure jet mill and with both temperature and pH gradients set but without ultrasound linkage control; 3-1 is a normal NFC orange juice control sample; 3-2 is the final peeled, full-component NFC orange juice sample obtained in Example 1. The descending overflow tank in this experimental example is formed by the weir crest height of the overflow weir plate decreasing gradually along the juice flow direction, the same applies below.
[0088] Each sample was added to a 2mm rectangular sample cell of a LUM and tested using a LUMiFuge stability analyzer. The test conditions were: detection wavelength 865nm, rotation speed 3000r / min, temperature 25℃, acquisition interval 10s, acquisition of 300 sets of spectra, total detection time 2990s; analysis interval width 10.00mm, reference transmittance 90%.
[0089]
[0090] Table 5. Data Analysis Interval Table for LUMiFuge Stability Test in Experiment Example 2 Table 5 lists the data analysis intervals used to calculate the instability index for each sample in Experiment 2's LUMiFuge stability test. An analysis interval of 10.00 mm was selected for each sample, with a reference transmittance of 90% and a detection time set to 3000 s. The detection channels in the table correspond to... Figure 6 The sample channel number is shown in the results table; the instability index reading time is 2990s, which is the final calculation time output by the instrument software. Figure 6 The Instability Index is an index of instability. Figure 6 The upper graph shows the trend of the instability index of each sample changing with the detection time. Figure 6 The lower bar chart represents the instability index of each sample at 2990 s. The smaller the instability index, the slower the change in transmittance of the sample under centrifugation acceleration conditions, and the better its suspension stability.
[0091]
[0092] Table 6. LUMiFuge stability test results of peeled full-component NFC orange juice under steady-state conditions of different gradient overflow tanks in Experiment Example 2. In Table 6, RCA represents the average relative centrifugal acceleration, derived from... Figure 6 As shown in Tables 5 and 6, all samples in Experiment 2 underwent LUMiFuge stability testing using a 10.00 mm analysis interval, 90% reference transmittance, and a detection time of 3000 s. The instability index of the optimized sample 3-2 obtained in Example 1 was 0.219, lower than the instability index of the ordinary NFC orange juice control sample 3-1 (0.685), and also lower than the instability index of sample 1-1 (0.675), which was only treated with 100 MPa high-pressure jet milling but did not enter the gradient overflow tank. Compared with sample 1-1, the instability index of sample 3-2 decreased by approximately 67.6%; compared with the ordinary NFC orange juice control sample 3-1, the instability index of sample 3-2 decreased by approximately 68.0%. These results indicate that the overflow path above the descending weir after high-pressure jet milling, the temperature / pH gradient, and the linkage of low-intensity pulsed ultrasound are beneficial to improving the suspension stability of peeled whole-component juice.
[0093] Experiment Example 3: Verification Experiment Based on the Optimization Conditions of Experiment Example 2 This experimental example is used to illustrate... Figure 7 How was the LUMiFuge stability data obtained? Experiment 3 used the same raw material processing, wet pre-grinding, viscosity adjustment, and 100MPa high-pressure jet mill conditions as Experiment 2, focusing on comparing the stability of the optimized gradient overflow tank sample with several samples that deviated from the conditions.
[0094] Sample 3-3 is the final peeled, full-component NFC-type orange juice sample obtained by repeating Example 1; Sample 4-1 is a sample treated with only 100MPa high-pressure jet milling without entering the gradient overflow tank; Sample 4-2 is a sample treated with 100MPa high-pressure jet milling and then entering the horizontal flow tank without a descending weir; Sample 4-3 is a sample treated with 100MPa high-pressure jet milling and then entering the descending overflow tank without a cooling and shaping chamber; Sample 5-1 is a sample with only a pH gradient and no temperature gradient; Sample 5-2 is a sample with a temperature / pH gradient but no upper overflow path; Sample 5-3 is a sample with a temperature / pH gradient but using continuous high-intensity ultrasound; Sample 6-1 is a sample treated with 100MPa high-pressure jet milling and then entering a normal temporary storage tank.
[0095] The test conditions were the same as in Experiment 2: wavelength 865nm, rotation speed 3000r / min, temperature 25℃, acquisition interval 10s, acquisition of 300 sets of spectral lines, total detection time 2990s; analysis interval width 10.00mm, reference transmittance 90%.
[0096]
[0097] Table 7. Data Analysis Interval Table for LUMiFuge Stability Verification Test in Experiment Example 3 Table 7 lists the data analysis intervals used to calculate the instability index for each sample in Experiment 3 during the LUMiFuge stability verification test. An analysis interval of 10.00 mm was selected for each sample, with a reference transmittance of 90% and a detection time set to 3000 s. The detection channels in the table correspond to... Figure 7 The sample channel number in the results table; the instability index reading time is 2990s. Figure 7 The upper graph shows the trend of the instability index of each sample changing with the detection time. Figure 7 The lower bar chart represents the instability index of each sample at 2990 s. The smaller the instability index, the slower the change in transmittance of the sample under centrifugation acceleration conditions, and the better its suspension stability. Figure 7 The Instability Index represents the instability index. Figure 7 This was used to compare the stability differences between optimized gradient overflow tank samples and samples that deviated from the conditions of lacking descending weirs, lacking cooling and shaping, lacking upper overflow paths, using continuous high-intensity ultrasound, or only undergoing ordinary temporary storage treatment.
[0098]
[0099] Table 8. LUMiFuge stability verification test results of peeled full-component NFC orange juice under different stabilization treatments in Experiment Example 3. In Table 8, RCA represents the average relative centrifugal acceleration. Figure 7As shown in Tables 7 and 8, all samples in Experiment 3 underwent LUMiFuge stability verification testing using a 10.00 mm analysis interval, 90% reference transmittance, and a detection time of 3000 s. The instability index of the replicated Sample 3-3 from Example 1 was 0.152, significantly lower than the instability index of Sample 4-1 (treated only by high-pressure jet mill, 0.725), and also lower than the instability index of Sample 4-2 (without descending weir, 0.618), Sample 4-3 (without cooling and shaping chamber, 0.753), Sample 5-1 (with only pH gradient, 0.691), Sample 5-2 (without upper overflow path, 0.658), Sample 5-3 (continuous high-intensity ultrasonic, 0.750), and Sample 6-1 (ordinary temporary storage tank, 0.646). Compared to sample 4-1, the instability index of sample 3-3 decreased by approximately 79.0%; compared to sample 6-1 in a conventional temporary storage tank, the instability index of sample 3-3 decreased by approximately 76.5%. These results further demonstrate that the improved stability is not solely attributable to the high-pressure jet mill or conventional temporary storage, but rather to a combination of factors including the overflow path above the descending weir after the high-pressure jet mill, gradient temperature, gradient pH, cooling and shaping, and low-intensity pulsed ultrasound.
[0100] Experiments 2 and 3 show that the peeled whole-component NFC orange juice obtained in Example 1 exhibits a low instability index in the LUMiFuge centrifugation accelerated stability test. Specifically, the instability index of the optimized sample 3-2 from Example 1 in Experiment 2 is 0.219, and the instability index of the verified sample 3-3 in Experiment 3 is 0.152, both significantly lower than samples subjected to deviating conditions such as high-pressure jet milling, ordinary temporary storage tank, no descending weir, no upper overflow path, no cooling and shaping, or continuous high-intensity ultrasound. This demonstrates that the present invention, through the combination of high-pressure jet milling for fine dispersion and subsequent gradient overflow tank for stabilization assembly, can promote the formation of a stable suspension network of endogenous pectin, pulp fiber, cell wall particles, juice sac fragments, and aroma oil droplets in peeled whole-component orange juice, thereby improving the suspension stability of the final product.
[0101] Experimental Example 4: Basic Evaluation of Pressure and Particle Size in High-Pressure Jet Mill This experimental example illustrates why the high-pressure jet mill pressure is preferably set to 100 MPa in Example 1. The samples in Example 4 were prepared as peeled, full-component fruit pulp according to S1 to S7 of Example 1, but without entering the gradient overflow tank. The high-pressure jet mill pressures were set to 60 MPa, 80 MPa, 100 MPa, and 120 MPa, respectively. NFC orange juice control, crushed and degassed samples, and 1:1 viscosity-adjusted samples were also included.
[0102] After high-pressure jet milling, each sample underwent evaluation using the LUMiFuge instability index, centrifugal sedimentation rate, and laser particle size analyzer. The test results were used to determine the pressure of the high-pressure jet mill as a pre-treatment refining and dispersion step, rather than to evaluate the final stability of the subsequent gradient overflow tank.
[0103] like Figure 8 As shown, the instability index varies among samples with different jet pressures and viscosity-adjusting ratios, with samples treated near 100 MPa exhibiting better stability. Figure 9 The results show that the average particle size of the samples generally decreases with increasing jet pressure. Figure 8 and Figure 9 100 MPa can be considered the preferred pressure point for the high-pressure jet mill refining activation step in Example 1. It should be noted that Experiment 4 only demonstrates that the high-pressure jet mill can provide the necessary refining basis; the final product stability still needs to be evaluated through the combination of the high-pressure jet mill and the gradient overflow channel in Example 1.
[0104] Experimental Example 5: Evaluation of Dietary Fiber and Total Component Retention This experiment was used to evaluate the dietary fiber retention of the peeled, full-component NFC orange juice prepared in Example 1. Three types of samples were used: regular NFC juice, concentrated reconstituted juice, and the peeled, full-component NFC orange juice prepared in Example 1. Equal volumes or masses of each sample were thoroughly mixed, and the total dietary fiber, soluble dietary fiber, and insoluble dietary fiber content were measured.
[0105] Figure 10 In the figure, the horizontal axis is divided into three groups according to the detection indicators: "Total," "Soluble," and "Insoluble." "Total" represents the total dietary fiber content, "Soluble" represents the soluble dietary fiber content, and "Insoluble" represents the insoluble dietary fiber content. Each group includes three types of samples: "Peeled Whole Fruit Juice," "NFC," and "Concentrate." "Peeled Whole Fruit Juice" corresponds to the peeled whole-component NFC orange juice prepared in Example 1, "NFC" corresponds to ordinary NFC juice, and "Concentrate" corresponds to concentrated reconstituted juice. Figure 10 The vertical axis, "Relative abundance of Dietary Fiber / (g / 100ml)", represents the dietary fiber content, expressed in g / 100mL, indicating the mass of dietary fiber per 100mL of sample. In the graph, "ns" indicates no significant difference, "*" indicates a significant difference, and "**" indicates an extremely significant difference.
[0106] Depend on Figure 10As can be seen, the peeled, full-component NFC orange juice prepared in Example 1 has higher total dietary fiber and insoluble dietary fiber content than the concentrated reconstituted juice, and maintains a high level compared with ordinary NFC juice; the soluble dietary fiber content shows relatively small differences among the three samples. This result indicates that the dietary fiber advantage of the product in this application mainly stems from the retention of insoluble structural components such as pulp fiber, cell wall particles, and juice vesicle fragments. This application utilizes high-pressure jet milling for fine dispersion and gradient overflow tank for stabilization assembly, enabling the full-component particles containing dietary fiber to form a stable suspension network, thereby improving suspension stability while retaining the full-component properties of the peeled orange pulp.
[0107] The present invention relates to the processing, transmission and reception procedures of controllers, ultrasonic auxiliary units, ultrasonic generators, pH monitors, pH adjustment devices, temperature monitors, temperature control devices, etc. These are conventional technical choices for those skilled in the art, belong to the prior art, and are technical solutions that can be obtained without creative effort, and are not the subject matter protected by the present invention.
[0108] The above embodiments should be understood as illustrative only and not as limiting the scope of protection of the present invention. After reading the description of the present invention, those skilled in the art can make various alterations or modifications to the present invention, and these equivalent changes and modifications also fall within the scope defined by the claims of the present invention.
Claims
1. A method for the preparation of a gradient-flooded, stabilized, peeled, full- component NFC-type orange juice, characterized by, Includes the following steps: S1. Oranges are subjected to enzymatic peeling to obtain peeled orange pulp with the peel removed but the juice vesicles, pulp fibers, cell wall particles and endogenous pectin retained. S2. The peeled orange pulp is wet-pre-pulverized, and NFC orange juice base viscosity-adjusting liquid is added during and / or after pre-pulverization to mix and adjust viscosity, so as to obtain peeled whole component fruit pulp with the peeled orange pulp as the main component. S3. The peeled whole-component fruit pulp is subjected to high-pressure jet milling to refine and evenly disperse the juice cell fragments, pulp fibers, cell wall particles, endogenous pectin and aroma oil droplets in the peeled whole-component fruit pulp, thereby obtaining refined whole-component fruit juice. S4. The refined whole-component juice is introduced into a gradient overflow tank for stabilization treatment. The gradient overflow tank is provided with multiple overflow chambers connected by an upper overflow method along the juice flow direction. Each of the multiple overflow chambers includes at least a heating activation chamber, a guiding assembly chamber, and a cooling and shaping chamber. The multiple overflow chambers are respectively configured with temperature and pH control conditions to form a gradient temperature and gradient pH along the juice flow direction. The refined whole-component juice flows through the heating activation chamber, the guiding assembly chamber, and the cooling and shaping chamber in sequence by overflow, thereby causing the endogenous pectin, pulp fiber, cell wall particles, juice cell fragments, and aroma oil droplets to gradually assemble into a stable suspended network and be discharged from the cooling and shaping chamber to obtain stable peeled whole-component NFC orange juice.
2. The production method according to claim 1, characterized by, The heating activation chamber, the guiding assembly chamber, and the cooling and shaping chamber are respectively configured with the following temperature and pH conditions: The temperature of the heating and activation chamber is 35℃-55℃, and the pH is 3.3-4.
0. It is used to reduce the viscosity of the juice system and promote the contact between endogenous pectin, pulp fiber and cell wall particles. The temperature of the guided assembly chamber is 20℃-40℃ and the pH is 3.6-4.5, which is used to promote the formation of a networked suspension structure of endogenous pectin, pulp fiber, cell wall particles, juice cell fragments and aroma oil droplets under overflow thin layer and guided flow conditions. The cooling and shaping chamber has a temperature of 4℃-25℃ and a pH of 3.4-4.2, and is used to cool and shape the already formed networked suspension structure.
3. The production method according to claim 2, characterized by, The gradient overflow tank includes an inlet buffer chamber, a heating activation chamber, a guiding assembly chamber, and a cooling and shaping chamber, which are arranged sequentially along the juice flow direction and connected by an upper overflow method; an overflow weir plate is provided between two adjacent overflow chambers; after the refined whole-component juice reaches a predetermined liquid level in the previous overflow chamber, it crosses the corresponding overflow weir plate and enters the next overflow chamber; the cooling and shaping chamber is provided with a discharge port, through which the shaped peeled whole-component NFC orange juice is discharged; The inlet buffer chamber is configured with temperature and pH conditions: the temperature of the inlet buffer chamber is 15℃-45℃ and the pH is 3.0-4.5, which is used to buffer the feed pressure, flow rate and temperature fluctuations of the refined whole-component juice.
4. The production method according to claim 3, characterized by, The outlet of the cooling and shaping chamber is located on the side away from the inlet of the cooling and shaping chamber; the outlet is a rounded, slow-flow outlet, and the shaped peeled, full-component NFC orange juice is discharged through the rounded, slow-flow outlet by gravity flow due to liquid level difference and / or assisted by a low-speed volumetric pump; the outlet is connected to a food-grade discharge pipeline, and the average flow velocity of the juice in the food-grade discharge pipeline is 0.05 m / s-1.0 m / s; when a low-speed volumetric pump is used to assist in the discharge, the low-speed volumetric pump is one of a cam rotor pump, a peristaltic pump, a diaphragm pump, or a single screw pump.
5. The preparation method according to claim 3, characterized in that, The inlet buffer chamber, heating activation chamber, guiding assembly chamber, and cooling shaping chamber are formed by multiple overflow weir plates within the same tank body, or by multiple independent tank bodies connected in series through upper overflow ports, overflow pipes, or overflow weir plates.
6. The preparation method according to claim 3, characterized in that, The inlet buffer chamber, heating activation chamber, guiding assembly chamber, and cooling and shaping chamber are all equipped with pH monitors and pH adjustment ports, as well as temperature monitors and temperature control devices. The pH is adjusted by food-grade acid, food-grade salt, or their buffer system, and the food-grade acid, food-grade salt, or their buffer system includes one or more of citric acid, citrate, malic acid, and malate.
7. The preparation method according to claim 3, characterized in that, The gradient overflow tank also includes an ultrasonic auxiliary unit for performing low-intensity or pulsed ultrasonic assisted treatment on the refined whole-component juice; the ultrasonic auxiliary unit includes an insertable ultrasonic probe disposed in at least one overflow chamber of the inlet buffer chamber, the heating activation chamber and the guide assembly chamber, and / or an externally coupled ultrasonic transducer disposed outside at least one overflow chamber of the inlet buffer chamber, the heating activation chamber and the guide assembly chamber. The insertion ultrasonic probe includes an amplitude transformer and an ultrasonic tool head, wherein the ultrasonic tool head extends into the working liquid level of the corresponding overflow chamber as the sound output end. The externally coupled ultrasonic transducer is installed on the wall, bottom or outer sleeve of the corresponding overflow chamber, and transmits ultrasonic energy to the juice inside the corresponding overflow chamber through the wall, bottom or outer sleeve. The insertable ultrasonic probe and / or externally coupled ultrasonic transducer are respectively connected to the corresponding ultrasonic generator or multi-channel ultrasonic generator, and are linked to the temperature monitor of the corresponding overflow chamber for control. When the juice temperature in the corresponding overflow chamber exceeds the upper limit of the overflow chamber temperature by 1℃-3℃, the output power of the corresponding insertable ultrasonic probe or externally coupled ultrasonic transducer is reduced, or the ultrasonic output is paused.
8. The preparation method according to claim 7, characterized in that, When the inlet buffer chamber, heating activation chamber, and guide assembly chamber are equipped with the insert-type ultrasonic probe and / or externally coupled ultrasonic transducer, the ultrasonic auxiliary parameters of the corresponding overflow chamber are as follows: The ultrasonic frequency of the entrance buffer chamber is 20kHz-30kHz, the sound power density is 0.02W / cm²-0.15W / cm², and the duty cycle is 5%-20%. The ultrasonic frequency of the heating activation chamber is 20kHz-35kHz, the sound power density is 0.05W / cm²-0.30W / cm², and the duty cycle is 10%-30%. The ultrasonic frequency of the guide assembly chamber is 20kHz-40kHz, the sound power density is 0.15W / cm²-0.60W / cm², and the duty cycle is 20%-50%.
9. The preparation method according to claim 1, characterized in that, In step S1, the ratio of oranges to enzymatic hydrolysate is 1:2-3, the pH of the enzymatic hydrolysate is 3.5-4.5, the amount of enzyme added is 1‰-4‰ of the mass of the enzymatic hydrolysate, and the enzymatic peeling time is 40min-60min; in step S2, the wet pre-grinding is a two-stage wet pre-grinding, and the rotation speed of both the first-stage and second-stage wet pre-grinding is 3000r / min-5000r / min; the NFC orange juice base viscosity is NFC orange juice, or a mixture of NFC orange juice and water, and the NFC orange juice accounts for more than 50% of the mass of the NFC orange juice base viscosity, and the water is used as an auxiliary viscosity-adjusting component; in step S3, the pressure of the high-pressure jet milling treatment is 60MPa-120MPa.
10. A peeled, full-component NFC orange juice, characterized in that, The peeled, full-component NFC-type orange juice is prepared by the preparation method according to any one of claims 1 to 9; the peeled, full-component NFC-type orange juice contains a stable suspension network formed by endogenous pectin, pulp fiber, cell wall particles, juice sac fragments and aroma oil droplets; under the LUMiFuge test conditions of detection wavelength 865nm, rotation speed 3000r / min, temperature 25℃, acquisition interval 10s, acquisition of 300 sets of spectra, and total detection time 2990s, the instability index of the peeled, full-component NFC-type orange juice is not higher than 0.30.
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